Sodium Hydroxide → 11-Hydroxy-11-methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic Acid

HRID 894217노트

반응식

HRID 894217 반응식
[OH:1][C:2]1([CH3:21])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([O:19]C)=[O:18])=[CH:16][C:3]1=2.[OH-].[Na+]>C(O)C>[OH:1][C:2]1([CH3:21])[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([OH:19])=[O:18])=[CH:16][C:3]1=2

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 21162722Methyl 11-hydroxy-11-methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate

생성물 1

HCID 1292913211-Hydroxy-11-methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylic Acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Dissolve 450 mg. of methyl 11-hydroxy-11-methyl-6,11-dihydrodibenz[b,e]oxepin-2-carboxylate in 20 ml. of ethanol and add 20 ml. of 5% aqueous sodium hydroxide solution. Stir at room temperature for 1 hour. Evaporate the alcohol and dilute the residual sodium salt solution with 40 ml of water. Cool in an ice bath and acidify with 5N hydrochloric acid. Separate the solids by filtration and dry (yield 250 mg). Recrystallize from benzene to obtain the title product (yield 200 mg., m.p. 258°-258° C.).

후처리

  1. dissolutionDissolve 450 mg
  2. customEvaporate the alcohol
  3. additiondilute the residual sodium salt solution with 40 ml of water
  4. temperatureCool in an ice bath
  5. customSeparate the solids
  6. filtrationby filtration
  7. customdry (yield 250 mg)
  8. customRecrystallize from benzene

출처 및 근거

ORD 기록
ord-f8f3a18c970e4f9bbcacf8918a22c125
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282365

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